Process of making hexachlorethane



the payment Patented Apr. 14, 1931 UNIT-ED STA GEORGE mavnnnn :BAn'rtnr'r, rnocnss on Maxine No Drawing. Application filed Mayfi,

res,

1925. Serial No. 29,233.

(GRANTED UNDER THE A031 01' MARCH 3, 1883, AS AMEIlDEIl) APRIL 30,.1928 370 0. G.'757).

This invention relates to a process of making hexachlorethane from carbon tetrachloride. 'Among the objects of this invention is 5 the provision of a process of making practically pure (3 Gb, which process is highly elficient, simple and easy to operate and which employs readily available materials.

A further object of this invention is to 1 provide a process of making GgCl. whereinv a valuable by-product is also obtained.

A still further object ofthis invention consistsdn a process of making 0 61 from- C01 and a metal, for example aluminum,

: the reaction being carried out in the pres,-

ence of a halide of aluminum, for example aluminum chloride.

In carrying out my invention, I introduce metallic aluminum and aluminumchloride into carbon tetrachloride heat the mixture condense vapors formed by the heating and reflux or return the condensed liquids to the mixture. I have found that f a small I amount of aluminum chloride is added to 5 a mixture of CO1. and metallic'aluminum and the mixture warmed tom-70? C., the reaction proceedsvery satisfactorily accord ing to the following equationi i 6CCl -+2Al+ (AlCl 3C Cl +2AlCl (A101 It will be observed that the small amount of A101 added to the. reactionmixture ap-,\

pears in the. final reaction'product and thereis also produced a' substantial amount of j A101,; by the reaction.

ThezCCl is employedin excess of the" quantity required in the reaction with the metallicaluminum and this excess should "minum chloride, thatreatment-of the product be 'suflic ient to dissolve the by the reaction. I This invention described herein maybe manufactured and used" byg or for the Gov? -ernment for Government purposes, without to me of any royalty'-thereon.-.

3 01 produced A specific examplefiof carryin out 'my I process i as followsz'Abput -1000*1bs. of

QChis' run into a reaction vessel, 34 lbs. of/ metallic aluminum and 5 lbs. of A1019 are added and the mixture, is heated.- The carried on at atmospheric pressure, 1s rephysical condition of the a'lu minum ,inflti ences the speed ofreaction and the quantity of materialproduced and "I have found that the proportion of 33 pounds of aluminum pellets and 1 pound of aluminum powder gives the best results. i It should be understood, however, that these proportions may be altered and other forms of. aluminum employed without departing from this invention. The reaction is conducted preferably at 75 (3., and is continuedfor about 18 to 24 hours or until the reaction, as

shown by control analysis, is practically complete. During this reaction the CCl. is subjected, to condensation and the liquids condensed thereby returned to the mixture which is agitated so that the small amount of gummy byproducts are removed from the metal, the aluminum pellets thus presenting a clean surface for reaction. Owing to the excess of CChemployed, there remains unreacted a sufiicient quantity of this re-agent to serve as a'solvent for'the C CL, produced. This solution of C Cl in CO1. is then filtered, ,thusiseparating the. A101 therefrom, and the filtrate is distilled by ordinary heating; The CCL. that is, removed by this distillation, which may be covered forfurthenuse. ","T-he remaining crude Q 01 is then "distilled with steam andcondensed in a! Waterfspray. This distilled product is then filtered from the water and d iied, i .5

The AlCl previouslymecoveredfrom the reaction product; may be Washed; wi h C01 and then purified by sublimation and con- 1 g densation. e

If it is not desired to recover the 3111-,-

after the reflux condensation has been oompleted may be modified ,b addin a quantity. of water to the react onpro uct suflicient to deconfpose the .AlCiQp- After this decom osition has taken place, the solution (Ill in CClymay bedrawn oil and then distilled, as heretofore described.

Although in. the foregoing example l haveillustrated the use of aluminum, it is to be understood that my invention is not and'in view of the numerous modifications .to 75 C., condensing which may be effected therein without departing from the spirit and scope of this invention, it is desired that only such limitations be imposed as are indicated in the appended claims.

I claimas my invention;

1. A process of making hexachlorethane comprising introducing metallic aluminum and a halide of aluminum into carbon tetrachloride and subjecting the mixture to a temperature suflicient to cause the formation of hexachlorethane. i

,2. A rocess of making hexachlorethane. comprising introducing metallic aluminum and aluminum chloride into carbon tetrachloride and subjecting the mixture to a temperature sufiicicnt to cause the formation of hexachlorenthane:

3. A recess of making hexachlorenthane comprislng introducin metallic aluminum and. alumlnum chloride into carbon tetrachloride and heating the mixture at from 60 to 75 C. I

4. A roc'ess of making hexachlorethane comprislng introducing metallic aluminum and a halide of aluminum into carbon tetrachloride, heating the mixture at from 60 to 75 CL, condensmg vapors formed by said heating and returning the condensed liquids to the mixture.

*5. A recess of making hexachlorethane comprising introducin metallic aluminum and aluminum chlori e'into carbon tetrachloride, heating the mixture at from 60 vapors formed b said heating and returning the condensed liquids to the mixture.

6. A process of making hexachlorethane 1 comprising introducing metallic aluminum and a halideof aluminum into carbon tetrachloride, the carbon tetrachloride being Eresent in suflicient excess'to dissolve the exachlorethane formed by the reaction, heatin s the mixture, condensing vapors forme bysaid heating, returning the condensed liquids to the mixture, separating the solution of, hexachlorethane in carbon tetrachloridefrom the other'products of the a reaction mixture and then distilling the carbon. tetrachloride from. said solution.

7. In a process of making I thane' com rising introducing metallic aluminum an aluminum chloride into carbon tetrachloride, thecarbon tetrachloride be-' 'ing present in suflicient excess to dissolve the hexachlorethane formed by the reaction, heatin the mixture, condensing vapors forrhe thereby, returning the condensed tion of hexachlorethane in tion mixture,

liquids tothe mixture, separating-the soluride from the other products of the reaction mixture, distilling the carbon tetrachloride from said solution and then distilling by means of steam, the crude hexachlorethane carbon tetrachloremaining after the carbon tetrachloride has been removed.

8. In a process of making hexachlorethane comprising introducing metallic alu minum and a halide of aluminum into carbon tetrachloride, the carbon tetrachloride being present in sufficient excess to dissolve the hexachlorethane formed by the reaction,- heating the. mixture, condensing vapors formed b said heating and returning the condense liquids to the mixture, separating the solution of hexachlorethane in carbon tetrachloride from the other products of the reaction mixture,( listilling the carbon tetrachloride from said solution, then distilling by meansof steam the crude hexachlorethane remaining after the carbon tetrachloride has been removed and condensing in a water spray the hexachlorethane evolved.

9. In a process of making hexachlorethane comprising introducing metallic aluminum and aluminum chloride into carbon tetrachloride, the carbon tetrachloride being present in sufficient excess to dissolve the hexachlorethane formed by the reaction, heating the mixture, condensing vapors formed" thereby, returning the condensed liquids to the mixture, separating the solution of hexachlorethane in carbon tetrachloride from the other products of the reac- 4 distilling the carbontetrachloride from said solution, then distilling by means of steam the crude hexachlorethane remaining after the carbontetrachloride has been removed, and condensing in a water L spray the hexachlorethane evolved, se aratlng the water from the condensate an drying the hexachlorethane.

10. In a process of making hexachlore-v thane com rising introducing metallic aluminum an tetrachloride, subjectingthe mixture to a temperature suflicient to cause the formation of hexachlorethane and agitating the mixture.

GEORGE MAYNARD BARTLETT.

a halide of aluminum into carbon 

